Process of making metallic oxids.



No. 846,444. PATENTED MAR. 12, 1907. J. W. BAILEY. PROCESS OF MAKING METALLIC OXIDS.

APPLICATION FILED MAR. 12 1902.

. 2 SHEETSSHEET 1.

WITNESSES: I INVENTOR/ BY L No. 846,444. v PATENTED MAR. 12, 1907.

- J. W. BAILEY.

PROCESS OF MAKING METALLIC OXIDS.

APPLICATION FILED MAR. 12, 1902.

2 SHEETS-SHEET 2.

WITNESSES: INVENTOR UNITED STATES PATENT OFFICE.

JOHN W. BAILEY, or JERSEY CITY, "NEW JERSEY, ASSIGNOR, BY MESNE Specification of Letters Patent.-

LEAD COMPANY, A CORPORATION OF NEW PROCESS OF MAKmemETALuc OXIDS.

' Patented March 12, 1907.

application filed March 12, 1902. Serial No- 97,s4s.

To (all whom, it may concern:

Be it known that 1, JOHN W. BAILEY, a' citizen of the United States, and a resident of Jersey City, in the county of Hudson and State of New'Jersey, have invented a certain new and useful Improved Process of Making Metallic Oxids, of which the following is a specification.

My invention relates to a process of making metallic oxids, and more especially to a proc: ess of making lead oxids for. use as pigments.

The process commonly employed heretofore for making the oxids of lead consists in exposing a mass of the molten metal in a reverberatory furnace to-the products of combustion of the fuel mixed with more or less air, the metal being continuously stirred'to expose fresh surraces to the action of the oxidizing agents. Leadhas also been oxidized-by placing the metal in a finely-divided state in a revolving cylinder through which the products ofcombustion of an adjoining furnace are conducted. In the'case of zinc the common process has been to volatilize the metal either rrom a molten mass or it or from the decomposition of itsores, the metallic vapor being burned to producethe oxid. Each of these processes is,v owing. among other things, to the form in which the metal is treated, slow and tedious and requires-a large expenditure of 11161. lhe product,

more'over, is more or less impure, being cont aminated with earthy and other matters from the fuel, and it is recovered in a i'orm which requires washing, grinding, and other treatment be ore it is fit ror use.

My invention has for anobject to provide a process of makingmetallic oxids which is simple and easily carried into eflect and every step of which, especially the oxidation of the metal, is rapidly perrormed and is under erfect control, also one which may be process.

manner, as by blowing a jet of steam or compressed air through a stream 01 the molten metal, can be iurther reduced to a very fine dust or impalpable powder by means of a suitable pulverizing or attrition mill and when thus finely divided can be quickly and economically reduced to the state of an oxid by'being exposed to the action of a current or hot air or of hot air and moisture. When the metallic powder is thus treated in a closed muflie that is suitably heated Without subjecting the metal to the action-of the products of combustion, a purer product is produced which is or a superior quality and is in a suitable condition ror'use without iurther treatmentsuch as grinding, washing, &c. and this product is produced in much less time than is required to carry out the pro-.

cesses 1n common use.

In order that my inventlon may be fully understood, re.'eren'ce 1s made to the accompanying drawings, in which is illustrated one .orm or apparatus by which my invention may be carried into effect, it being understood that my process is not restricted to the use of the apparatus which I am about to describe or to any particular apparatus or means of performing the various steps or the I Of the drawings, Figure 1 is a vertical longitudinal central sectional view of a suitable rorm or apparatus devised by me for carrying my process into effect, said apparatus forming the subject-matter 05 a companion application, Serial No. 97,849,filed March 12,

1902. Fig. 2 is a vertical transverse section o; theapparatus, taken on the line 2 2 of Fig. 1; and big. 3 is a sectional view illustrating a detail.

Like reference-numerals refer to like parts wherever-they occur throughout the drawings. 1

This apparatus-ccnsists, essentially, in the COIIlbiIlf L'Edt n,with a closed muflile,of means for heating the same, means for maintaining a current ofair in the muffle, means for introducing finely-comminuted metal into one end of the mufiie, means for advancing the metal therethrough, and a discharge-passage for the oxidized or partly-oxidized metal communicating with the other end of the muffle. In accordance with the preferred form of the apparatus there is also provided means for supplying moisture to the interior of the muflle and for agitating the metal as it is advanced therethrough. In the best embodiment of the apparatus a plurality of muflles are provided, the same being arranged to communicate with each other in series. In order that this series of mufiles may be suitably heated and maintained at progressively-increasing temperatures, they are arranged one above another in a suitable furnace, the means for introducing the metal being connected to the upper muflie of the series and the discharge-passage for the oxid. being connected to the lower mufile' of the series. The means for supplying the moisture consists of a series of steam-jets, one for each muflie, arranged in the air-supply passage so as to act at the same time to induce a current of air through each muffle and to suitably heat the air as it is introduced.

Referring to the drawings in detail, 1 represents the inclosing walls of asuitable furnace, and 2 represents the grate-bars therer of, to which the fuel is supplied through a suitable opening 3.

4 is the uptake or escape-pipe for the products'of combustion.

In the apparatus shown three muffies 5, 6,

. and 7 are provided, each consisting of a horizontally arranged longitudinally tapering shell which is fixed at its opposite ends in the walls of the furnace, the various muflles of the series being, as regards their taper, alternatelyarranged in reverse positions. For

the purpose of supplying air to the muflles air-passages 8, 9, and 10 are provided in one of the walls of the furnace, one passage for each of the muflles. In each of these airpassagesi's' provided an injector-nozzle, said nozzles being numbered, respectively, 11, 12, and 13. duced by these injector-nozzles may be suitably heated and at thesame time supplied with a suitable amount of moisture, the injector-nozzles are preferably connected to a steam-supply pipe 14, which is provided with a suitable regulating-valve 15.

17 represents a supply reservoir or hopper for the finely-divided metal, said hopper communicatin at its lower end with the su ply-pipe 18, w 1ich passes down through t e top of the furnace and enters the upper muffle 5, near the small end thereof, as shown. In the supply-pipe 18 is mounted a suitable feeding device, the same consisting in the construction shown of a wheel or cylinder 19, which, as shown in Fig. 3, is fitted to a suitable chamber in the supply-pipe and is pro vided with one or more circumferential re cesses 20, adapted upon the revolution of the Wheel to supply the finely-comminuted metal to the mufflein regulated quantities.

For the purpose of agitating the metal in the muflles,.so as to thoroughly and uniformly expose all the parts thereof to the air in the In order that the currents of air-in made successively longer from one end of each of the shafts to the other, so that their ends will all come in close proximity to the interior walls of the muflies. In order that the blades may act to advance the metal through the mufHes, as well as to agitate the same, the blades are preferably flattened at their ends and arranged at such an angle to the axis of the shafts as to advance the metal with which they come in contact to a greater or less amount, dependent upon the speed of rotation of the shaft. This advancing movement of the metal is also facilitated somewhat by the inclination of the bottoms of the muffles, due to their tapering form. The

shafts 22, 23, and 24 are driven by any suitable means, that shown consisting of a pulley 25 on the upper shaft and the gears 26, 27, and 28, which transmit the motion of the upper shaft 22 to the lower'shafts 23 and 24.

29 indicates a suitable outlet-passage for the oxidized metal, the same communicating at one end with the larger end of the lower muffle 7 and at the other end with a suitable receptacle 30 for the finished product.

In order that the metal may be supplied to the muifles in automatically-regulated quantitles, the feeding-cylinder 19 is mounted, on

a shaft 31, which is journaled in suitable;

bearings 32 and is provided at one end with a gear 33, which meshes with the gear 26 on the shaft 22. g I

34 indicates an escape-pipe for the air supplied to the mufiles by the air-passages 8, 9, and 10, provision being thus made to maintain a continuous currentthrough each of themufl'les. The pipe 34 preferably communicates near the small end of the upper muffle 5, and in'order that any particles of the metallic dust or of the oxid which is carried out by the current of air may be recovered the air-pipe 34 should terminate in a dust-settling chamber which, as it forms no part of my present invention, and as may be of any of the usual constructions, is not shown or described herein.

, In Fig. 2 is indicated a form of pulverizing- A discharge-pipe 46 communicates with an muffles, eachof them 1s provided with a suit 1 enlarged chamber 47, formed at the top of the casing 38. The discharge-pipe 46 communicates with the suction-port of a suitable blower 48, the delivery-port of which is connected by a suitable ber 17.

In accordance with my process the metallic lead is reduced in the mill described to such a fine state that it Will be floated in the air and carried thereby to a suitable settling chamber, which may be the supply-chamber 17 of the oxidizing apparatus. The heat of the furnace is so regulated that the upper retort 5 is maintained at a temperature some what below that at which the metal fuses. The lower mufiies 6 and 7 are preferably maintained at a somewhat higher temperature than that of the upper mufi'le 5, and the lowest muffle, in which the lead has all been changed to the form of an oxid, maybe maintained at ,a temperature considerably higher than that at which the metal fuses; but it should not be heated to such a temperature as to fuse'the oxid therein. I The supply of steam to the injector-nozzles is so a'djusted as to supply such a quantity of air and moisture to the mufiles as will cause the metallic particles to become gradually oxidized, and the speed of rotation of the agitating devices is so regulated as to advance pipe 49 to the chamthe metal through the mufiles at such a rate of speed that when the metal reaches the outlet-passage it will be oxidized to the desired extent. if, for instance, it is desired to produce litharge, (13b0,) the agitating devices will be run at such a speed that the metal will have been oxidized to that extent only when it is discharged. If,'however, it is desired to produce red lead, (Pb O the agitating devices will be operated at a slower speed, so that the lead will be further oxidized to the desired extent. The degree of oxidation and the rapidity thereof may of course be also regulated more or less by varying'the temperature of the furnace and by varying the temperature and the amount of the steam and air supplied to the chambers, it being within the judgment and skill of the operator to determine which of these elements of regulation can best be made use of to produce the desired result. Ifdesired, moreover, additional heating devices may be provided for increasing the temperature of the air supplied to the inufiles. Such heating devices are shown in Fig. 2 wherein 8, 9 and 10 indicate air-supply pipes which pass through the furnace and communicate with the air-supplygfpassages 8, 9, and 10, re-

spectively. Cut.- 8", 9 and 10 are provided to close the outer ends of the passages 8 9, and 10when it is desired to use the supplemental heaters. In fact, all of the heat provided to expedite the oxidation of the metalmay be supplied to the air, if desired.

. If desired, moreover, additional putlet-passages for the product may be provided, the

same being arranged to communicate with various parts of the muflles in order to dis- .charge the metal. therefrom when it has reached the desired degree of oxidation. Such a passage is indicated at 35 in Fig. 1, the same communicating at one end with the larger end of the intermediate muffle 6 and at the other end with a suitable receptacle 36. The passage between mufl'les 6 and 7 is closed by a cut-off 37 when the oxid is to be de livered from muffle 6. I

It is obvious that a greater or less number of the muffles may be used, if desired.

It will be observed that in accordance with my invention the process of oxidation of the metal is a gradual one and under perfect control from start to finish. Owing principally to the fine condition of the metal, however, it

is oxidized more rapidly and more uniformly than by the processes heretofore in common use. The product, moreover is discharged from the apparatus in a very pure and finely- .divided or amorphous condition and is ready for use without further treatment.

What I claim as new, and desire tosecure by Letters Patent, is

1. The process of making an oxid of a metal, which process consists in reducing the metal to an impal able'metallic powder and then slowly oxidizing the powder by heating it in the presence of an oxidizing. agent.

2. The process of making an oxid of a metal, which process consists in reducing the metal to an impalpable metallic powder and then oxidizing the powder by subjecting it to the action of heated air.

3. The process of making an oxid of" a metal which process consists in reducing the metal to an impalpable metallic powder and then subjecting the powder to the action of an oxidizing agent in such manner as to oxidize the metal without vaporization of the oxid.

4. The process of making a'n oxid of a metal, which process consists in reducing the metal to an'impalpable metallic Ipowder and then subjecting the powder to t e action of heated air in such manner as to oxidize the metal without vaporization of the oxid.

5. The process of making an oxid of ,a metal, which process consists in reducing the metal to an impalpable metallic powder and then heating the powder in a closed chamber to a temperature below the fusingoint of the metal and at the same time su jecting the metal to the action'of an oxidizing agent.

6. The process of making an oxid of me-.

tallic lead suitable for pigment, said process consisting in reducing the lead to an impal pable metallic owder and then slowly oxidizing the pow er.

7. The process of making an oxid of metallic lead suitable for pigment, said process consisting in reducingthe lead to an impalpable metallic powder and then slowly oxisame tlme su metal, which consists in heating the metaldizing the powder by subjecting it to the action of a heated oxidizing agent.

8. The process of making an oxid of metallic lead suitable for pigment, said process consisting in reducing the lead to an impalpable metallic powder and then subjecting the powder to the action of an oxidizing agent in such manner as to oxidize themetal without vaporization of the oxid.

9. The process of making an oxid of metallic lead suitable for pigment, said process consisting in reducing thelead to an impalpable metallic powder and then heating the powder in a closedchamber to a temperature elow the fusing-point of the metal and at the same time subjecting the metal to the action of an oxidizing agent.

10. The process of making an oxid of a metal, which process consists in reducing the metal to an impalpable metallic owder,

heating. the powder in the presence 0 an ox1- dizing'agent, and agitating the powder to uniformly expose all parts thereof to the oxidizing agent.

11. The process of making an oxid of a metal, which consists in reducing the metal to an impalpable metallic powder and then heating the powder in the presence of air and moisture. 1

12. The process of making an oxid of a metal, which consists in reducing the metal to an impalpable metallic powder and then heating the powder in the presence of a current of air and steam.

13. The rocess of making an oxid of, a metal whic heating the powderin a muffle and at the jecting it to the action of a current of heated air and steam. v v 14. The process ofmaking an oxidl of a in the form of an im alpable powder to a temperature below t e fusing-point in a closed muflle and at the same time subjecting the metal to the action of a current of heated air.

15. The process: of making an oxid of .a .metal, which consists in heating the metal in the form of an impal able powder to a tem-' perature below the sing-point in a closed muflie and 'at' the same time subjecting the 'metal to the action of a current of heated air and steam.

16. The rocess of making an oxid of a metal, whic consists heating the metal in the form of an impalpable powder to a temperaturebelow the fusing-point in a closed muflie and at the same time agitating the metal, which metal and subjecting the metal to thaaction ofa current of heated air.

17. The process of making ature below the fusing-point in a closed mufconsists in reducing the metal to an impalpable metallic powder. and then an oxid of a nslsts in heating the metal inthe form of an impalpable power to a temper-' fie and at the same time agitating the metal and subjecting the metal to the action of a current of heated air and steam.

18. The process of making an oxid of a metal, which rocess consists in heating the metal in the orm of an impalpable powder in such manner as to'gradually transform the metal into the character of oxid desired.

19. The process of makingan oxid of a metal, which process consists in gradually oxidizing the metal in the form of an impalpable powder by subjecting the powder to the action of an oxidizing agent and-moisture.

20. The process of making an oxid of a metal, which consists in subjecting the metal in the form of an impalpable powder to the action of a current of air and moisture heated to a temperature lower than that at which the metal fuses.

21. The process of making lead oxid suitable for pigment, said process consisting in reducing the lead to an impalpable metallic powder and then heating the powder in the presence of air and moisture.

22. The process of making lead oxid suitable for pigment, said process consisting in reducing the lead to an impalpable metallic powder and then heating the powder to a temperature below the fusing-point of the metal in the presence of air and moisture.

23. The process of making an oxid of a metal, which consists in reducing the metal to an impalpable metallic powder, fe'eding the powder and steam into a heated mufile in regulated quantities and subjecting the powder to the action of a current of heated air.

24. The process of making an oxid of a metal, which consists in reducing the -metal 'to an impalpable metallic powder, feeding the powder and steam in regulated quantities into a closed muflile heated to a temperature below the'fusin g-point of the metal, agitating the powder in the ,mufile and at the same time subjecting the powder to the action of a current of heated air.

metal whch consists in reducingthe metal to an impalpable metallic powder and then subjecting the powder to a gradually-increasing ture. a Y I g 7 26. The process of making an oxid of ametal which consists inreducingthemetalto an impalpable metallic powder and then sub ecting the powder to a gradually-increasing temperature in the presence of a current of heated air andsteam. 27. The process Ofmaking-anpxid ofa metal which consists in reducing the metalto an impalpable metallic powder, then heating the powder'to a'tem'perature below the fusing point of the metal the presence of air, and

then 'as the metal ibp'comes oxidized increasing' the temperature thereofg j 25. The process of making an oxid of a 28. The process of making an oxid of a metal which consists in reducing the metalto an impalpablemetallic powder, then heating the powder to a temperature below the fusingpoint of the metal in the presence of air and moisture, and then as the metal-becomes oxidized increasing the temperature thereof.

29. The process of making lead oxid, which process consists in heating the lead in the form of an impalpable powder in such manner as to gradua ly transform the lead into the character of oxid desired. 

